Process for preparing exchange silicates for industrial purposes



Patented July 1, 12%.

JAMES B. WHEBRY, 01E MDMOBE, SOUTH UTA.

IPROCESS FOR PREPARING SEICATES FOR INDUSTRIAL PURPOSES.

and useful Improvements in Processes for Pre aring Exchange Silicates for Industria Purposes, of which the following is a, specification.

My invention relates to the treatment, for commercial or industrial use, of that class of exchange silicates found in nature, which possess water softening properties.

The natural state of the raw material to be treated is usually that of clayey substance consisting of a hydrated silicate of aluminum which contains alkalis and alkaline earths, together with a small percentage of iron compounds includin iron silicates. Such raw material (found 1n parts of the United States) possesses exchange properties to a greater or less degree and may after treatment be used for removing the calcium and magnesium salts, usually termed the hardening salts, from water, or for any other purpose for which base exchange silicates may be adapted. While it is true that the natural silicates referred to have the property of base exchange, nevertheless it is not practical to use them commercially in their natural state because in that state these clayey substances resolve themselves into compact masses through which liquids' cannot readily or'rapidly filter. Moreover, in the natural state the raw material referred 'to contains a large percentage of microscopic particles which are fine enough to render the material colloidal in character. Furthermore, the natural material has mechanically mixed therewith foreign matter, which is soluble and therefore objectionable, and the proportion of alkalis and alkaline earths varies.

With the above factors in view it is a primary object of my invention to provide a novel and eflicient process for treating naturally occurring clays in such a manner that they will have a uniform chemical composition and be free from objectionable foreign matter which originally was mixed therewith.

A further object is to adapt the plastic colloidal raw material to formhard granules of convenient size,which will not disintegrate when placed in water, but will retain 1922. Serial 110. 567,825.

the base exchange properties of the original substance. c

It is also my object to correct theproportions of alkalis and alkaline earths present in the natural exchange silicates by adding predetermined and proper amounts of alkalis or alkaline earths and a salt of sodium or potassium to a slurry of the natural silicates before drying or reducing the mass to granules of suitable size.

In my improved process 11 first make a slurry of the naturally occurring clay and remove the mechanically mixed foreign matter and then by the addition of suitable reagents (hereinafter described) bring the clay approximately to the following composition: Combined water (above 110 deg. C.) 7.10 Silicon dioxide 57.23 Iron oxide 3.50 Aluminum oxide 24.70 Manganese dioxide Calcium oxide 2.50 Magnesium 0xide. 2.16 Sodium oxide 1.71 Potassium oxide Sulphur trioxide .10 Hydrogen sulphide Carbon dioxide Chlorides .38

The substances in the natural or raw clay which vary largely and must be corrected are the calcium and magnesium, To correct these substances in a given batch, the raw clay is analyzed and if the content of these important substances varies materially from the proportions given above an approprlate amount of the deficient substance-is added.

In a given batch, for example, it might be found that there is insufficient calcium.

In this case a 6% solution of 'a soluble loo added. One or more salts of alkali metals, 5 or the alkaline earth metals mentioned above are thus added (from 2 to 10% by weight as determined by analysis of the natural clay) to correct by chemical exchange the proportions of the bases present. In this are with v inate a After the introduction of the desired percentage of a salt or salts of alkali or alkaline earth metals I consider it desirable, although not essential to my invention, to pass the material thus rectified through a thickener of any suitable kind, which serves to elimconsiderable part of the water in the slurry and also to wash away impurities in the solution. Whatever excess water may then remain over that desired for the production of a plastic, easily working mass is removed by suitable filters and at this point a water wash is used to further loidal forms a net work mg the heat treatment cient hardness so that remove soluble impurities and the excess of the salts used for rectifying.

The plastic mam resulting from the treatment amve described is now forced through .dies of suitable size and pressed into long string-like forms, loosely termed noodles, which are conveyed 01' carried into low temperature dryers. Here the greater part of the free moisture isremoved and the resultant particles rendered of sufiithey may be ground and classified as desired, into granules. This drying step, though desirable in most cases, may be omitted, all of the moisture being expelld as follows: The dried particles re-' sulting from the treatment in the low temperature dryers or. if desired the plastic noodles from the dies .are next subjected to a heat treatment which may be referred to as a baking step, the temperature at this stage of the process being suficiently high to completely dehydrate the material without fusing it. That is to say, this last mentloned step isintended to remove all of the ,water of constitution as well as the chemically combined Water so that the particle are completely dehydrated but the heat aplied is not sufiicient to cause fusion of the rticles. An important and distinctive feature of this bahng step is that it oom-' pletely dehydrates the colloidal matter to which the plasticity of the raw material is ue and renders the granules rigid and nonoohesive. Thus the matter which was colof reinforcement throughout th particles which is not destroyed by the subsequent treatment.

To indicate to the operator when the proper temperature has been reached durit is preferable, though not essential that a small amount about 2%) of sodium chloride be added to t e slurry-before the drying is commenced.

hydrate the same and the step of first weaves hours, or until the reaction is completed.

The purpose of this rehydrating step is to remove any excess silica and restore the chemically combined water lost by the heat treatment, thus reviving the chemical properties of the material so that it will function as a base exchange material and will give up its sodium content for the calcium or magnesium content in hard water, or vice versa.

As a final step the hydrated material is washed free from excess alkali hydroxides and insoluble impurities, thus placing it in condition for use for Water softening or other industrial purposes.

Having described my invention what T claim as new and desire to protect by Letters Patent is: i

1. The method of producing granulated zeolite from natural clay which comprises first producing a slurry from the clay then alkalizing the slurry to correct the quantity of bases present, then reducing the mass to dry particles by heating to a. temperature sufficiently high to completely dehydrate the same and subsequently rehydrating the dried particles.

2. The method of producing granulated zeolite from natural clay which comprises first producing a slurry from the clay then.

alkalizing the slurry, then reducing the mass to dry particles by heating to a temperature sufiiciently high to completely desubsequently rehydrating with an alkali-metal hydroxide.

3. The method of producing granulated zeolite from natural clay which comprises first producing a slurry from the clay then alkalizing the slurry to correct the quantities of bases present and adding a 2% solution of sodium chloride then reducing the mass to dry particles, by heating to a temperature sufficiently high to completely dehydrate the same and subsequently rehydra-ting the dried particles to render them capable of softening water.

4:. The method of making base exchange silicates from natural clay which includes producing a slurry, addin to the slurry an alkali earth-metal salt, and removing mechanically mixed foreign matter, subsequently removing from the slurry the greater part of the water content thereof leaving a plastic mass, then forming the plastic mam into particles, then heating the particles to a temperature sufliciently high to completely dehydrat the same and hydrating the material to render it capable 15 finally rehydrating the material to render it of softening water. capable of softenin water. 6. The method of roducing granulated 5. The method 0 making base exchange zeolite from natural clay which consists in,

5 silicates from natural clay which comprises alkalizing the clay to correct the quantities first producing a, slurry, alkalizing the of bases present, then reducing the mass to 20 slurry to correct the quantities of bases particles and heating to a temperature sufiipresent, re'inovin from the slurry the water ciently high to completely de-hydrate the content thereof caving a plastic mass, then same and subsequently re-hydrating the '10 reducing the lastic mass into string-like particles to render them capable of softenparticles and r ing and formin granules in water; 26 thereof, then su jecting the drie particles 11 testimony whereof, I have hereunto to a temperature sufliclently high to comsigned my name to this specification.

pletely dehydrate the same and finally re- JAMES B. WHERRY. 

